TAN Gaohao, WANG Chengye, ZHENG Jinming, et al. Simultaneous Determination of 37 Veterinary Drugs in Animal-Derived Foods by Ultra-high Performance Liquid Chromatography-tandem Mass Spectrometry(UPLC-MS/MS)[J]. Science and Technology of Food Industry, 2021, 42(17): 225−234. (in Chinese with English abstract). doi: 10.13386/j.issn1002-0306.202009030.
Citation: TAN Gaohao, WANG Chengye, ZHENG Jinming, et al. Simultaneous Determination of 37 Veterinary Drugs in Animal-Derived Foods by Ultra-high Performance Liquid Chromatography-tandem Mass Spectrometry(UPLC-MS/MS)[J]. Science and Technology of Food Industry, 2021, 42(17): 225−234. (in Chinese with English abstract). doi: 10.13386/j.issn1002-0306.202009030.

Simultaneous Determination of 37 Veterinary Drugs in Animal-Derived Foods by Ultra-high Performance Liquid Chromatography-tandem Mass Spectrometry(UPLC-MS/MS)

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  • Received Date: September 28, 2020
  • Available Online: June 14, 2021
  • A method for the determination of 37 veterinary drugs in animal-derived foods with QuEChERS by UPLC-MS /MS was established. The sample was extracted by 1% formic acid-acetonitrile precipitated protein, purified by PSA, C18, NH2 adsorbent. The separation was performed on Waters ACQUITY UPLC BEH C18 (1.7 μm, 2.1 mm×100 mm) column. The mobile phase performed on 0.1% formic acid aqueous solution-methanol by gradient elution, electrospray ionization source (ESI) was applied and operated in the positive mode. Multiple reaction monitoring (MRM) mode was used to monitor ions. Matrix matching standard curve quantification by external standard method. Results showed that, an excellent linear relationship in the range of 1.0~200 μg/L was observed for all the analytes with a correlation coefficient larger than 0.9980. The recoveries at three concentrations ranged from 70.1% to 97.7%, with the RSD from 0.9% to 5.6%. The limits of quantification of the method were 0.01~0.54 μg/kg. This method was used to detect 152 batches of animal-derived food samples which purchased at the farmer’s market. Sulfadiazine and trimethoprim were detected in 3 batches of Oreochromis mossambicus, the remaining samples were not detected. The method was simple, rapid and had good precision, accuracy and quantitative limit. It would be suitable for the rapid determination of nitroimidazoles and their metabolites, sulfonamides in animal-derived foods.
  • [1]
    陈振桂, 占春瑞, 郭平, 等. 高效液相色谱法同时测定水产品中13种磺胺类药物残留的研究[J]. 食品科学,2007(28):448−451. [Chen Z H, Zhan C R, Guo P, et al. Study on simultaneous determination of 13 sulfonamides residues in aquatic products by HPLC[J]. Food Science,2007(28):448−451. doi: 10.3321/j.issn:1002-6630.2007.10.111
    [2]
    Wulf N R, Matuszewski K A. Sulfonamide cross-reactivity: Is there evidence to support broad cross-allergenicity?[J]. American Journal of Health System Pharmacy,2013,70:1483−1494. doi: 10.2146/ajhp120291
    [3]
    Ilardi E A, Vitaku E, Njardarson J T. Data-mining for sulfur and fluorine: An evaluation of pharmaceuticals to reveal opportunities for drug design and discovery[J]. Journal of Medicinal Chemistry,2014,57:2832−2842. doi: 10.1021/jm401375q
    [4]
    殷居易, 谢东华, 刘永明, 等. 蜂产品中9种硝基咪唑类药物原药及代谢物残留量的HPLC-APCI(+)MS/MS分析[J]. 分析测试学报,2009,28(8):935−939. [Yin J Y, Xie D H, Liu Y M, et al. Determination of nitroimidazole drug residues in bee products by liquid chromatography-atmospheric pressre chemical ionization-tandem quadrupole mass spectrometry[J]. Journal of Instrumental Analysis,2009,28(8):935−939. doi: 10.3969/j.issn.1004-4957.2009.08.013
    [5]
    Kantiani L, Llorca M, Sanch S J, et al. Emerging food contaminants: A review[J]. Analytical & Bioanalytical Chemistry,2010,398(6):2413−2427.
    [6]
    Pessel D, Jagadeshwar-Reddy T, Verdon E. Develop-ment of a new screening method for the detection of antibiotic residues in muscle tissues using liquid chromatography and high resolution mass spectrometry with a LC-LTQ-Orbitrap instrument[J]. Food Additives & Contaminants,2011(10):1340−1351.
    [7]
    晏利芝, 赵永彪, 富玉, 等. 超高效液相色谱-串联质谱法同时测定猪肉中β-受体激动剂、喹诺酮类和磺胺类兽药残留量[J]. 分析试验室,2011,30(1):84−86. [Yan L Z, Zhao Y B, F Y, et al. Simultaneous determination of β-agonist, quinolones and sulfonamides residues in pork by ultra performance liquid chromatography-electrosp ray ionization tandem mass spectrometry[J]. Chinese Journal of Analysis Laboratory,2011,30(1):84−86. doi: 10.3969/j.issn.1000-0720.2011.01.024
    [8]
    王浩, 赵丽, 杨红梅, 等. 液相色谱-串联质谱法测定牛奶中35种四环素类、磺胺类、青霉素类、大环内酯类、氯霉素类抗生素残留[J]. 色谱,2015,33(9):995−1001. [Wang H, Zhao L, Yang H M, et al. Determination of 35 antibiotic residues of tetracyclines, sulfonamides, penicillins, macrolides and amphenicols in milk by liquid chromatography-tandem mass spectrometry[J]. Chinese Journal of Chromatography,2015,33(9):995−1001. doi: 10.3724/SP.J.1123.2015.04046
    [9]
    Aguilera-Luiz M M, Vidal J L M, Romero-Gonz Lez R, et al. Multiclass method for fast determination of veterinary drug residues in baby food b ultra-high-performance liquid chromatography-tandem mass spectrometry[J]. Food Chemistry,2012,132(4):2171−2180. doi: 10.1016/j.foodchem.2011.12.042
    [10]
    祖恩慧, 张岚, 于龙飞. 3种硝基咪唑类药物治疗滴虫性阴道炎的有效性及不良反应研究[J]. 中国妇幼保健,2015,30(12):1936−1938. [Zu E H, Zhang L, Yu L F. Study on the effectiveness and adverse reactions of three nitroimidazoles in treatment of trichomonas vaginitis[J]. Maternal and Child Health Care of China,2015,30(12):1936−1938.
    [11]
    农业农村部, 国家卫生健康委员会, 国家市场监督管理总局. GB 31650-2019中国食品安全标准食品中兽药最大残留限量[S]. 北京: 中国标准出版社, 2019.

    Ministry of Agriculture and Rural Affairs Announcement, National Health Commission, State Administration for Market Regulation. GB 31650-2019 Naional food safety standard. Maximum residue limits for veterinary drugs in foods[S]. Beijing: National Standards Press, 2019.
    [12]
    Won S Y, Chang H L, Chang H S, et al. Monitoring of 14 sulfonamide antibiotic residues in marine products using HPLC-PDA and LC-MS/MS[J]Food Control, 2011, 22: 1101-1107.
    [13]
    Meng Z, Shi Z, Liang S, et al. Residues investigation of fluoroquinolones and sulphonamides and their metabolites in bovine milk by quantification and confirmation using ultra-performance liquid chromatography-tandem mass spectrometry[J]. Food Chemistry,2015,174:597−605. doi: 10.1016/j.foodchem.2014.11.067
    [14]
    刁志祥, 王旭堂, 张培杨, 等. 动物源性食品中磺胺类药物和β-受体激动剂残留的色谱和质谱检测技术研究进展[J]. 中国畜牧杂志,2020,56(5):12−19. [Diao Z X, Wang X T, Zhang P Y, et al. Research progress on chromatographic and mass spectrometric detection techniques for sulfonamides and beta-agonist residues in animal-derived foods[J]. Chinese Journal of Animal Science,2020,56(5):12−19.
    [15]
    汪纪仓, 马素英, 王大菊, 等. 气相色谱-离子阱串联质谱法同时测定猪肌肉中硝基咪唑类药物残留[J]. 畜牧兽医学报,2008,39(12):1772−1778. [Wang J C, Ma S Y, Wang D J, et al. Simultaneous determination of nitroimidazole residues in swine meat by gas chromatography-ion trap tandem mass spectrometry[J]. Acta Veterinaria et Zootechnica Sinica,2008,39(12):1772−1778. doi: 10.3321/j.issn:0366-6964.2008.12.023
    [16]
    张鸿伟, 简慧敏, 林黎明, 等. 液相色谱-四极杆/离子阱质谱快速测定蜂蜜中痕量硝基咪唑类药物及其代谢物残留[J]. 分析测试学报,2012,31(7):763−770. [Zhang H W, Jian H M, Lin L M, et al. Rapid detection of trace amounts of nitroimidazoles and their metabolites in honey using liquid chroma tography coupled with quadrupole /linear ion trap mass spectrometry[J]. Journal of Instrumental Analysis,2012,31(7):763−770. doi: 10.3969/j.issn.1004-4957.2012.07.002
    [17]
    潘娟, 严凤, 张婧, 等. 超高效液相色谱-静电轨道阱质谱同时筛查测定猪肉中21种磺胺类药物残留[J]. 上海畜牧兽医通讯,2019(4):8−13. [Pan J, Yan F, Zhang Q, et al. Simultaneous screening and determination of 21 sulfonamides residues in pork by ultra performance liquid chromatography-electrostatic orbital trap mass spectrometry[J]. Shanghai Journal of Animal Husbandry and Veterinary Medicin,2019(4):8−13.
    [18]
    Sun H, Qi H, Li H. Development of capillary electrophoretic method combined with accelerated solvent extraction for simultaneous determination of residual sulfonamidesand their acetylated metabolites in aquatic products[J]. Food Analytical Methods, 2013, 6: 1049-1055.
    [19]
    Zhang Y, Xu X, Qi X, et al. Determination of sulfonamides in livers using matrix solid-phase dispersion extraction high-performance liquid chrom atography[J]. Journal of Separation Science,2012,35:45. doi: 10.1002/jssc.201100600
    [20]
    Yu H, Mu H, Hu Y M. Determination of fluoroquinolones, sulfonamides, tetracyclines multiresidues simultaneously in porcine tissue by MSPD and HPLC–DAD[J]. Journal of Pharmaceutical Analysis,2012,2:76−81. doi: 10.1016/j.jpha.2011.09.007
    [21]
    Xie W, Han C, Hou J B, et al. Simultaneous determination of multiveterinary drug residues in pork meat by liquid chromatography-tandem mass spectrometry combined with solid phase extraction[J]. Journal of Separation Science,2012,35:3447−3454. doi: 10.1002/jssc.201200407
    [22]
    赵巧灵, 张薇英, 汤海凤, 等. 快速溶剂萃取-超高效液相色谱-串联质谱法测定养殖鱼肌肉中19种磺胺类药物残留[J]. 食品科技,2019,44(12):335−341. [Zhao Q L, Zhang W Y, Tang H F, et al. Determination of 19 sulfonamides residues in cultured fish muscle with accelerated solvent extraction by high performance liquid chromatography-tandem mass spectrometry[J]. Food Science and Technology,2019,44(12):335−341.
    [23]
    陈兴连, 林 涛, 刘兴勇, 等. 超高效液相色谱-串联质谱法快速测定鱼和虾中多类禁、限用兽药残留[J]. 色谱,2020,38(5):538−546. [Chen X L, Lin Tao, Liu X Y, et al. Rapid determination of multiple prohibited and restricted veterinary drugresidues in fish and shrimp by ultra high performance liquid chromatography-tandem mass spectrometry[J]. Chinese Journal of Chromatography,2020,38(5):538−546.
    [24]
    廖夏云, 杨黎, 刘星, 等. 蜂胶胶囊中多种硝基咪唑类药物残留的检测[J]. 现代食品科技,2020,36(5):295−303,191. [Liao X Y, Yang L, Liu X, et al. Determination the residues of nitroimidazoles in propolis capsules by LC-MS/MS[J]. Modern Food Science and Technology,2020,36(5):295−303,191.
    [25]
    郑璇, 张晓岭, 邹家素, 等. 超高效液相色谱-三重四极杆质谱法测定地表水和废水中的19种磺胺类抗生素[J]. 理化检验(化学分册),2018,54(6):680−687. [Zhen X, Zhang X L, Zou J S, et al. Determination of 19 sulfonamide antibiotics in suface water and waste water by ultra hight performance liquid chromatog-raphy-triple quadrupole mass spectrometry[J]. Physical Testing and Chemical Analysis (Part B: Chemical Analysis),2018,54(6):680−687.
    [26]
    励炯, 孙 岚, 王红青, 等. 分散固相萃取净化/高效液相色谱-串联质谱法测定水产品中的5种硝基咪唑类药物残留[J]. 分析测试学报,2017,36(11):1357−1362. [Li T, Sun L, Wang H Q, et al. Determination of five nitromidazoles in aquatic products by high performance liquid chromatography-tandem mass spectrometry combined with dispersive solid phase extraction[J]. Journal of Instrumental Analysi,2017,36(11):1357−1362. doi: 10.3969/j.issn.1004-4957.2017.11.011
    [27]
    Fedorova G, Nebesky V, Randak T, et al. Simultaneous determination of 32 antibiotics in aquaculture products using LC-MS/MS[J]. Chemical Papers,2014,68:29−36.
    [28]
    曲斌. QuEChERS在动物源性食品兽药残留检测中的研究进展[J]. 食品科学,2013,34(5):327−331. [Q B. Advances in application of QuEChERS for detection of veterinary drug residues in animal-derived foods[J]. Food Science,2013,34(5):327−331.
    [29]
    黄子敬, 王晓玲, 杨钦沾, 等. 超高效液相色谱-串联质谱法同时测定畜禽肉中磺胺类、喹诺酮类、硝基咪唑类兽药残留[J]. 分析试验室,2014,333(10):1184−1188. [Huang Z J, Wang X L, Yang Q Z, et al. Determination of sulfonamides, quinolones and nitroimidazoles in meat by ultra performance liquid chromatography-tandem mass spectrometry[J]. Chinese Journal of Analysis Laboratory,2014,333(10):1184−1188.
    [30]
    Won S Y, Chang H L, Chang HS, et al. Monitoring of 14 sulfonamide antibiotic residues in marine products using HPLC-PDA and LC-MS/MS[J]. Food Control,2011,22:1101−1107. doi: 10.1016/j.foodcont.2011.01.005
    [31]
    张虹艳, 邱国玉, 吴福祥, 等. 组织研磨-QuEChERS-高效液相色谱-串联质谱法测定动物源食品中磺胺类药物残留以及基质效应的研究[J]. 食品工业科技,2020,41(10):259−264,270. [Zhang H Y, Qiu G Y, Wu F X, et al. Determination of sulfonamides in animal-originated foods by grinder-QuEChERS-high performance liquid chromatolgraphy-tandem mass spectrometry and research on matrix effects[J]. Science and Technology of Food Industry,2020,41(10):259−264,270.
    [32]
    李蓉, 杨璐齐, 罗阳丹, 等. QuEChERS/UPLC-Q-Orbitrap HRMS法测定水产及水产加工品中16种苯并咪唑类与13种硝基咪唑类药物残留[J]. 分析测试学报,2018,37(5):547−555. [Li R, Yang L Q, Luo Y D, et al. Determination of 16 benzimidazoles and 13 nitroimidazoles residues in fish and fishery products by UPLC-Q-Orbitrap HRMS with QuEChERS[J]. Chinese Journal of Analysis Laboratory,2018,37(5):547−555. doi: 10.3969/j.issn.1004-4957.2018.05.005
    [33]
    国家质量监督检验检疫总局. SN/T 2624-2010 动物源性食品中多种碱性药物残留量的检测方法液相色谱-质谱/质谱法[S]. 北京: 中华人民共和国出入境检验检疫行业标准, 2010.

    General Administration of Quality Supervision. Inspection and Quarantine of the People's Republic of China. SN/T 2624-2010 Determination of several alkaline drug residues in animal food by liquid chromatography-mass spectrometry[S]. Beijing: Industry Standard for Entry-exit inspection and Quarantine of the People's Republic of China, 2010.
    [34]
    中华人民共和国海关总署. SN/T 1626-2019 出口肉及肉制品中甲硝唑、替硝唑、奥硝唑、洛硝哒唑、二甲硝咪唑、赛克硝唑残留量测定方法液相色谱-质谱/质谱法[S]. 北京: 中华人民共和国出入境检验检疫行业标准, 2019.

    General Administration of Customs, P, R, China. SN/T 1626-2019 Methods for the determination of metronidazole, tinidazole, ornidazole, lonidazole, dimetr-Imazole, and secnidazole residues in exported meat and meat products liquid chromatography-mass spectrometry[S]. Beijing: Industry Standard for Entry-exitins-pection and Quarantine of the People’s Republic of China, 2019.
    [35]
    中华人民共和国农业部. 农业部1025号公告-23-2008. 动物源食品中磺胺类药物残留检测液相色谱-串联质谱法[S]. 北京: 国家标准出版社, 2008.

    Ministry of Agriculture of the PRC. Ministry of Agriculture No. 1025-23-2008. Determination of sulfonamides residues in animal food by liquid Chromatography-mass spectrometry[S]. Beijing: National Standards Press, 2008.
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